CN103240053A - Corrosive sulfur removal agent for insulating oil and production method of corrosive sulfur removal agent - Google Patents
Corrosive sulfur removal agent for insulating oil and production method of corrosive sulfur removal agent Download PDFInfo
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- CN103240053A CN103240053A CN2013101834307A CN201310183430A CN103240053A CN 103240053 A CN103240053 A CN 103240053A CN 2013101834307 A CN2013101834307 A CN 2013101834307A CN 201310183430 A CN201310183430 A CN 201310183430A CN 103240053 A CN103240053 A CN 103240053A
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Abstract
The invention discloses a corrosive sulfur removal agent for insulating oil and a production method of the corrosive sulfur removal agent. The method adopts the following raw materials and comprises the following steps of: (1) performing the conventional ion exchange to a zeolite molecular sieve, nickel nitrate and water to obtain an adsorbent; (2) filtering the adsorbent and roasting to obtain a zeolite molecular sieve containing silicon and aluminum; (3) performing the conventional ion exchange to the zeolite molecular sieve obtained in the step (2), nickel nitrate and water to obtain another adsorbent, and drying the adsorbent to obtain corrosive sulfur removal agent powder for the insulating oil; (4) mixing the corrosive sulfur removal agent powder for the insulating oil, kaolin, water glass, sodium pyrophosphate and water; and (5) forming the mixed size obtained in the step (4) to obtain a finished product. The corrosive sulfur removal agent for the insulating oil is high in activity, can effectively prevent the oil from ageing, enables the simplification of the processing process, and is convenient for performing the work of removing corrosive sulfur at the site of a substation, and therefore, the corrosive sulfur removal agent has a potential economic benefit prospect.
Description
Technical field
The invention belongs to the insulating oil processing technology field, relate in particular to a kind of insulating oil active sulfur for removal insulation of electrical installation oil corrosivity sulfuration thing and remove agent and production method thereof.
Background technology
Insulating oil is a kind of petroleum refining product that comprises direct-connected alkane, cycloalkane and aromatic hydrocarbon, is widely used in electrical equipments such as transformer, transformer, breaker, can not only play insulating effect, also has the function of heat radiation, arc extinguishing and information carrier.The mercaptan that comprises in the insulating oil, disulphide etc. can cause the corrosion of transformer copper winding, can generate cuprous sulfide at coil surface after the long-time running, reduce the insulating properties of insulating paper, can cause transformer insulated layer to puncture when serious and burn.The thiophene sulfides that comprises in the insulating oil can not produce corrosiveness to copper, can also suppress oil deterioration, should continue to keep.Adopting the English full name of inductively coupled plasma atomic emission ICP-OES(is the abbreviation of " Inductively coupled plasma-optical emission spectroscopy ", and Chinese translation is " inductively coupled plasma atomic emission ".), a large amount of insulating oil total sulfur contents are detected, find that the sulfur content of tested insulating oil is in 100～1000ppm scope.Test method(s) GB/T25961-2010 according to active sulfur in the electric insulating oil detects insulating oil in service, and the result shows the situation ubiquity that contains active sulfur in the insulating oil.In the prior art, adopt the mode of adding matal deactivator usually, isolate active sulfur by the copper coil surface filming and solve the problem that contains active sulfur in the insulating oil.This method single treatment is convenient, effective, cost is low, but passivator can constantly consume in running, needs constantly to monitoring timely replenishing with insulating oil.For fundamentally solving insulating oil active sulfur problem, very be necessary corrosivity sulfuration thing in the oil is removed, to ensure the electrical equipment safe and stable operation, improve economic and social benefits.Be the Chinese patent literature introduction of CN102186959A according to publication number, Siemens Company is by using the lucium that adds salic-alumina silicate in the oil to transformer, and be heated to 300 ℃, the aqueous solution that adds soluble metal salt then cools off, be heated to 200 ℃ of maintenances at least two hours again, with the corrosive sulfur compounds in the neutralizing transformer usefulness oil.But such high-temperature process not only can cause the insulation oil deterioration to decompose, and its field processing equipment and treatment process have complicated and loaded down with trivial details suspicion.
Summary of the invention
The technical problem to be solved in the present invention is at the defective of prior art, to provide a kind of and remove agent and production method thereof for the insulating oil active sulfur of removing insulation of electrical installation oil corrosivity sulfuration thing.Require this adsorbent activity strong, have the selective absorption performance, can remove corrosivity sulfuration thing at a lower temperature, effectively prevent the oil ageing that high temperature causes.
Technical scheme of the present invention is, provides a kind of insulating oil active sulfur to remove agent and production method thereof, comprises adopting following raw material and step:
(1) (one or more in other nitrate as calcium, magnesium, nickel, cobalt, zinc, gold, silver, copper, iron, villaumite or the sulfate all can to get zeolite molecular sieve, nickel nitrate or nickel chloride or nickelous sulfate by weight 0.1-1:0.01-1:5-20 successively.), water carries out conventional ion exchange, wherein said zeolite molecular sieve institute siliceous with weight ratio aluminium be 1-100.Make the Na of described zeolite molecular sieve
2The weight percent content that the weight percent content of O reaches 1-5%, metal oxide reaches 1-25%, gets adsorbent.Conventional ion described in this step exchange refers to that the ion-exchange condition is room temperature to 100 ℃, adds acid solution control pH value in the 2.0-7.0 scope, and acid solution can be hydrochloric acid, sulfuric acid or salpeter solution, and be 0.5-24 hour ion-exchange swap time;
(2) filtration step (1) gained adsorbent was inserted 500-1000 ℃ of steam kiln roasting 1-10 hour with gained filter back adsorbent, and obtaining siliceous, aluminium weight ratio is the zeolite molecular sieve of 1-100;
(3) (one or more in other nitrate as calcium, magnesium, nickel, cobalt, zinc, gold, silver, copper, iron, villaumite or the sulfate all can to get step (2) gained zeolite molecular sieve, nickel nitrate or nickel chloride or nickelous sulfate by weight 0.1-1:0.01-1:5-20 successively.), water carries out conventional ion exchange, filter, again adsorbent.Will be again the gained adsorbent inserted in the 100-150 ℃ of environment dry 12-24 hour, get powder insulating oil active sulfur and remove agent.Conventional ion described in this step exchange refers to that the ion-exchange condition is room temperature to 100 ℃, adds acid solution control pH value in the 2.0-7.0 scope, and acid solution can be hydrochloric acid, sulfuric acid or salpeter solution, and be 0.5-24 hour ion-exchange swap time;
(4) successively by weight 0.1-1:0.01-0.1:0.01-0.03:0.01-0.02:5-20 get step (3) gained powder insulating oil active sulfur remove agent, solid binder kaolin or imvite or clay, liquid-containing binder waterglass or carboxymethyl cellulose, dispersant sodium pyrophosphate, water mix mixed serum;
(5) step (4) gained mixed serum is implemented spray drying forming processing or the processing of extrusion drying and moulding or balling-up drying and moulding and handle, namely get product insulating oil active sulfur of the present invention and remove the agent finished product.
Step (5) gained insulating oil active sulfur is removed agent, insert in the 20-100 ℃ of environment with the insulating oil that contains active sulfur and fully contact, can remove the active sulfur composition in the insulating oil that contains active sulfur, be 1-48 hour time of contact.Surplus used insulating oil active sulfur removes agent after finishing, and can insert under nitrogen purging condition and carry out conventional activating and regenerating processing in the 500-1000 ℃ of steam roaster, makes product insulating oil active sulfur of the present invention remove agent thus and obtains to recycle.
The invention has the beneficial effects as follows that the invention product is active strong, have the selective absorption performance, can remove corrosivity sulfuration thing at a lower temperature, effectively prevents the oil ageing that high temperature causes.Adopt insulating oil active sulfur of the present invention to remove agent and can simplify treatment process, very be convenient to carry out corrosivity sulfuration thing at the transformer station scene and remove work for the treatment of.These advantages of the present invention make the insulating oil active sulfur that produces remove agent and had wider range of application in actual promoting the use of, thereby have potential economic benefit expection.
The specific embodiment:
Embodiment 1:
(1) get zeolite molecular sieve 0.1 ㎏, nickel nitrate 0.01 ㎏, water 5 ㎏ and carry out the conventional ion exchange, wherein zeolite molecular sieve institute siliceous with weight ratio aluminium be 1-100.Make the Na of described zeolite molecular sieve
2The weight percent content that the weight percent content of O reaches 1-5%, metal oxide reaches 1-25%, gets adsorbent;
(2) filtration step (1) gained adsorbent was inserted 500-1000 ℃ of steam kiln roasting 1 hour with gained filter back adsorbent, and obtaining siliceous, aluminium weight ratio is the zeolite molecular sieve of 1-100;
(3) get step (2) gained zeolite molecular sieve 0.1 ㎏, nickel nitrate 0.01 ㎏, water 5 ㎏ and carry out the conventional ion exchange, filter, again adsorbent.Will be again the gained adsorbent inserted in the 100-150 ℃ of environment dry 12 hours, get powder insulating oil active sulfur and remove agent;
(4) get step (3) gained powder insulating oil active sulfur remove agent 0.1 ㎏, kaolin 0.01 ㎏, waterglass 0.01 ㎏, sodium pyrophosphate 0.01 ㎏, water 5 ㎏ mix mixed serum;
(5) processing namely gets the insulating oil active sulfur and removes the agent finished product to step (4) gained mixed serum enforcement spray drying forming.
Embodiment 2:
(1) get zeolite molecular sieve 1 ㎏, nickelous sulfate 1 ㎏, water 20 ㎏ and carry out the conventional ion exchange, wherein said zeolite molecular sieve institute siliceous with weight ratio aluminium be 1-100.Make the Na of described zeolite molecular sieve
2The weight percent content that the weight percent content of O reaches 1-5%, metal oxide reaches 1-25%, gets adsorbent;
(2) filtration step (1) gained adsorbent was inserted 500-1000 ℃ of steam kiln roasting 10 hours with gained filter back adsorbent, and obtaining siliceous, aluminium weight ratio is the zeolite molecular sieve of 1-100;
(3) get step (2) gained zeolite molecular sieve 1 ㎏, nickelous sulfate 1 ㎏, water 20 ㎏ and carry out the conventional ion exchange, filter, again adsorbent.Will be again the gained adsorbent inserted in the 100-150 ℃ of environment dry 24 hours, get powder insulating oil active sulfur and remove agent;
(4) get step (3) gained powder insulating oil active sulfur remove agent 1 ㎏, clay 0.1 ㎏, carboxymethyl cellulose 0.03 ㎏, sodium pyrophosphate 0.02 ㎏, water 20 ㎏ mix mixed serum;
(5) step (4) gained mixed serum is implemented the balling-up drying and moulding and handle, namely get the insulating oil active sulfur and remove the agent finished product.
Claims (1)
1. an insulating oil active sulfur removes agent and production method thereof, and this method comprises the following raw material of employing and step:
(1) successively by weight 0.1-1:0.01-1:5-20 get zeolite molecular sieve, nickel nitrate or nickel chloride or nickelous sulfate, water carries out the conventional ion exchange, wherein said zeolite molecular sieve institute siliceous with weight ratio aluminium be 1-100, make the Na of described zeolite molecular sieve
2The weight percent content that the weight percent content of O reaches 1-5%, metal oxide reaches 1-25%, gets adsorbent;
(2) filtration step (1) gained adsorbent was inserted 500-1000 ℃ of steam kiln roasting 1-10 hour with gained filter back adsorbent, and obtaining siliceous, aluminium weight ratio is the zeolite molecular sieve of 1-100;
(3) successively by weight 0.1-1:0.01-1:5-20 get step (2) gained zeolite molecular sieve, nickel nitrate or nickel chloride or nickelous sulfate, water carries out the conventional ion exchange, filter, get adsorbent again, will be again the gained adsorbent inserted in the 100-150 ℃ of environment dry 12-24 hour, get powder insulating oil active sulfur and remove agent;
(4) successively by weight 0.1-1:0.01-0.1:0.01-0.03:0.01-0.02:5-20 get step (3) gained powder insulating oil active sulfur remove agent, kaolin or imvite or clay, waterglass or carboxymethyl cellulose, sodium pyrophosphate, water mix mixed serum;
(5) step (4) gained mixed serum is implemented spray drying forming processing or the processing of extrusion drying and moulding or balling-up drying and moulding and handle, namely get the insulating oil active sulfur and remove the agent finished product.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105032024A (en) * | 2015-08-17 | 2015-11-11 | 国家电网公司 | Method for removing benzyl disulfide from dielectric oil |
| CN105126748A (en) * | 2015-08-14 | 2015-12-09 | 国网山东省电力公司临沂供电公司 | Transformer waste oil processing adsorbent and production method thereof |
| CN107446689A (en) * | 2017-08-08 | 2017-12-08 | 国网江苏省电力公司盐城供电公司 | A kind of restorative procedure of transformer insulation oil |
| CN107523408A (en) * | 2017-08-28 | 2017-12-29 | 国网江苏省电力公司电力科学研究院 | The chemical treatment method of active sulfur compound in a kind of elimination insulating oil |
| CN107638867A (en) * | 2017-10-24 | 2018-01-30 | 国网黑龙江省电力有限公司电力科学研究院 | A kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil |
| CN109603312A (en) * | 2019-01-25 | 2019-04-12 | 广东电网有限责任公司 | A kind of insulating oil active sulfur removing filter plate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1068049A (en) * | 1991-06-27 | 1993-01-20 | 吴凤义 | Purifying agent for insulating oil |
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2013
- 2013-05-17 CN CN201310183430.7A patent/CN103240053B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1068049A (en) * | 1991-06-27 | 1993-01-20 | 吴凤义 | Purifying agent for insulating oil |
Non-Patent Citations (1)
| Title |
|---|
| 王清清等: "Ni离子改性分子筛模拟柴油吸附脱硫的性能与机理", 《高校化学工程学报》, vol. 22, no. 6, 31 December 2008 (2008-12-31), pages 1049 - 1054 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105126748A (en) * | 2015-08-14 | 2015-12-09 | 国网山东省电力公司临沂供电公司 | Transformer waste oil processing adsorbent and production method thereof |
| CN105126748B (en) * | 2015-08-14 | 2018-07-31 | 国网山东省电力公司临沂供电公司 | Handle the adsorbent and its production method of transformer waste oil |
| CN105032024A (en) * | 2015-08-17 | 2015-11-11 | 国家电网公司 | Method for removing benzyl disulfide from dielectric oil |
| CN107446689A (en) * | 2017-08-08 | 2017-12-08 | 国网江苏省电力公司盐城供电公司 | A kind of restorative procedure of transformer insulation oil |
| CN107523408A (en) * | 2017-08-28 | 2017-12-29 | 国网江苏省电力公司电力科学研究院 | The chemical treatment method of active sulfur compound in a kind of elimination insulating oil |
| CN107638867A (en) * | 2017-10-24 | 2018-01-30 | 国网黑龙江省电力有限公司电力科学研究院 | A kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil |
| CN109603312A (en) * | 2019-01-25 | 2019-04-12 | 广东电网有限责任公司 | A kind of insulating oil active sulfur removing filter plate |
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Inventor after: Pan Hua Inventor after: Wan Tao Inventor after: Zhou Zhou Inventor after: Zhou Weihua Inventor after: Feng Bing Inventor after: Qian Hui Inventor after: Gong Shangkun Inventor before: Wan Tao Inventor before: Qian Hui Inventor before: Feng Bing Inventor before: He Tiexiang Inventor before: Gong Shangkun Inventor before: Zhou Zhou Inventor before: Chang Yan Inventor before: Liu Xiaoling |
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